Aborted
crsexp012scheme.jpg

Researcher

Cuepil Choi

Objective

To see if carrying out CRSEXP006 with a benzene ethylene glycol azeotrope and benezene water azeotrope in a rotary device with suction could help isolate and crystalize the acetal products.

Procedure

Ethylene glycol and 4-chlorobenzaldehyde were mixed in a 1.2:1 ratio, respectively, in a 100 mL round flask. Enough benzene was added to the round flask until approximately 30 mL of solution was inside. The round flask was clamped onto a rotary device. Rotary device was turned on and weak suction applied. When most of the top benzene layer escaped the round flask into the second chamber, additional benze was added. Samples were taken every time benzene was added after mixing through the rotary device.

Results


Conclusion

HNMR spectra showed little acetal production. Rotary device did not produce desirable results and further benzene additions were aborted.

Log

2013-07-26

11:20 mass of 100 mL round flask 1 65.193 g
11:24 1.081 g 4-chlorobenzaldehyde added to round flask 1
11:25 2.211 g ethylene glycol added to round flask 1
11:27 0.276 g g 4-chlorobenzaldehyde added to round flask 1
11:30 10.175 g of benzene added to round flask 1
11:35 two layers formed, S-1 taken from top benzene layer after mixing by rotating the rotary device
11:52 clear benzene layer goes cloudy
11:58 rotary device reaches 55 C upper round flask of rotary device starts to have a clear liquid
12:00 60 C reached on rotary device
12:19 rotary device turned off
12:22 10.085 g benzene add to round flask 1
12:26 rotary device back on
12:27 S-2 taken from top benzene layer
12:29 64 C reached on rotary device
12:34 top round flask on rotary device starts to have clear liquid
12:39 rotary device turned off
12:48 8.617 g of benzene added
12:53 S-3 taken from top benzene layer
13:30 HNMR spectrum 1 taken of S-1
13:50 HNMR spectrum 2 taken of S-2
13:56 HNMR spectrum 3 taken of S-3